反应详情

N-Bromosuccinimide (2.6 g) and 2,2′-azobis(isobutyronitrile) (35 mg) were added to a solution of 5-bromo-2-methylbenzotrifluoride (CAS #86845-27-4, 3.5 g) in carbon tetrachloride (35 mL), and the mixture was heated under reflux for five hours. The reaction solution was ice-cooled and then the insoluble matter was removed by filtration. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (carrier: Wakogel C-200; elution solvent: heptane) to obtain 3.86 g of the title compound. The property values of the compound are as follows.

1. temperaturethe mixture was heated
2. temperatureunder reflux for five hours
3. temperaturecooled
4. customthe insoluble matter was removed by filtration
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (carrier: Wakogel C-200; elution solvent: heptane)